Preparation method of tetraglycidyl m-xylene diamine epoxy resin

A technology of m-xylylenediamine epoxy resin and tetraglycidyl, which is applied in the field of preparation of tetraglycidyl m-xylylenediamine epoxy resin, can solve the problem of high viscosity and toxicity of m-xylylenediamine epoxy resin Large size, high cost, etc., to avoid hydrolysis and self-polymerization, reduce the content of organic chlorine, reduce the effect of resin viscosity

Active Publication Date: 2012-12-19
CHANGZHOU SUNCHEM HIGH FORMANCE POLYMER +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deficiency of this method is: because epichlorohydrin is easily hydrolyzed, self-polymerizes, and this is not well controlled again in this reaction process, causes the viscosity of the m-xylylenediamine epoxy resin that finally obtains is bigger (16500 ~20000mPa·S)
And the deficiency of its preparation tetraglycidyl amino compound is: ring closure reaction needs to adopt phase transfer catalyst, not only causes cost higher, and the onium salt compound and linear polyether compound that it adopts are also the catalyst of epoxy group ring opening, so in While catalyzing the ring-closing reaction, it will also increase the risk of resin self-polymerization, and the macrocyclic polyether compounds (that is, crown ethers) used are extremely expensive and highly toxic, and remain in water during post-treatment, greatly increasing the waste water. Difficulty and cost of processing

Method used

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  • Preparation method of tetraglycidyl m-xylene diamine epoxy resin

Examples

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Effect test

Embodiment 1）

[0018] The preparation method of the tetraglycidyl m-xylylenediamine epoxy resin of the present embodiment has the following steps:

[0019] ①Put 277.5g of epichlorohydrin (3mol) and 7.20g of deionized water (0.4mol) in sequence into a 1000mL four-necked flask equipped with mechanical stirring, reflux condenser, and thermometer, heat to 45°C, and in 1h Slowly add 27.2 g of m-xylylenediamine (0.2 mol) dropwise, and heat to 58° C. for 8 hours for ring-opening reaction.

[0020] ② Cool down to 45°C, add 66.67g of 48wt% sodium hydroxide solution (containing 32g of sodium hydroxide, 0.8mol) dropwise to the material obtained in step ① within 2h, and continue the ring-closing reaction at 45°C for 2h .

[0021] ③ After the reaction is finished, the epichlorohydrin is recovered by distillation under reduced pressure at a temperature of 60° C. for 1 hour. Then add 170mL of methyl isobutyl ketone and 170mL of water, stir slowly at a temperature of 60°C until completely dissolved, pour ...

Embodiment 2～ Embodiment 4）

[0028] The preparation method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.

[0029] Table 1

[0030] Example 1 Example 2 Example 3 Example 4 m-xylylenediamine 27.2g (0.2mol) 27.2g (0.2mol) 27.2g (0.2mol) 27.2g (0.2mol) Deionized water 7.2g (0.4mol) 7.2g (0.4mol) 7.2g (0.4mol) 7.2g (0.4mol) Epichlorohydrin 277.5g (3mol) 296g (3.2mol) 259g (2.8mol) 277.5g (3mol) The dropping temperature and time of m-xylylenediamine 45℃，1h 30℃，0.5h 50℃，1h 40℃，1h Ring opening reaction temperature and time 58℃，8h 60℃，6h 50℃，4h 45℃，4h alkaline solution 66.67g, 48wt% sodium hydroxide solution 150g, 30wt% potassium hydroxide solution 71g, 45wt% sodium hydroxide solution 64g, 50wt% sodium hydroxide solution Alkali solution dropping temperature and time 45℃，2h 60℃，3h 50℃，3h 55℃，2.5h Ring closing reaction temperature and time 45℃，2h 60℃，1.5h ...

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Abstract

The invention discloses a preparation method of tetraglycidyl m-xylene diamine epoxy resin, which comprises the following steps: (1) adding epichlorohydrin and deionized water into a reaction device, dropwisely adding m-xylene diamine for a ring-opening reaction; (2) adding an aqueous alkali into the material obtained in step (1) for a ring-closure reaction, wherein the molar ratio of the alkali in the aqueous alkali to the m-xylene diamine is 4:1; (3) after the reaction, recovering epichlorohydrin, adding an inert solvent and deionized water, performing extraction layering, removing the water layer; (4) refining the organic layer with the aqueous alkali, wherein the molar ratio of the alkali in the aqueous alkali to the m-xylene diamine is 1:1-2.5:1; (5) washing the refined material with water, removing the solvent to obtain the tetraglycidyl m-xylene diamine epoxy resin. The method of the invention is simple in process, easy to implement, and low in cost, and the prepared tetraglycidyl m-xylene diamine epoxy resin has low viscosity, low organic chloride content, and a high epoxy value.

Description

technical field [0001] The invention relates to a preparation method of a glycidyl amine epoxy resin, in particular to a preparation method of a tetraglycidyl m-xylylenediamine epoxy resin. Background technique [0002] Epoxy resin has been widely used in coatings, adhesives and other fields due to its good comprehensive mechanical properties, unique adhesion, excellent insulation, and small shrinkage. The glass transition temperature of general-purpose epoxy resin is 100°C-160°C, and the thermal deformation temperature is 70°C-140°C, so it cannot meet the requirements of high-temperature resistance applications such as aerospace electromechanical. [0003] Multifunctional epoxy resins (such as tetraglycidyl-4,4'-diaminodiphenylmethane, tetraglycidyl-4,4'-diaminodiphenyl ether, tetraglycidyl-3,4 '-diaminodiphenyl ether, etc.) Because the molecular structure contains four epoxy groups, the cured product has a high crosslinking density, a glass transition temperature of 230°C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/10
Inventor 胡和丰陆航方琳黄洪亮徐菁胡国宜吴建华华向阳蒋明跃沈国南
Owner CHANGZHOU SUNCHEM HIGH FORMANCE POLYMER
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